Levocarnitine compound and new preparation method thereof
A synthesis method and catalyst technology, applied in the field of levocarnitine compound and its new method, can solve the problems of cumbersome steps, low yield, expensive, etc.
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[0037] Example 1 Synthesis of (R)-4-chloro-3-hydroxy-butyric acid ethyl ester
[0038] Dissolve 165g (1mol) of ethyl 4-chloroacetoacetate in 300ml of ethanol, add it to the hydrogenation reactor, and then add 10g of L-tartaric acid modified Ni-B / SiO 2 Catalyst, airtight reactor, replace the air in the reactor with nitrogen, then blow in hydrogen to replace the nitrogen, keep the pressure of the reactor at 10kg, then increase the temperature and control the reaction at 60℃, react for 5 hours, leave to cool, and concentrate the reaction mixture under reduced pressure , The concentrate is distilled in high vacuum, and the fractions at 70°C (about 0.5mmHg) are collected to obtain 155g of colorless transparent liquid (R)-4-chloro-3-hydroxy-butyric acid ethyl ester, yield: 93%, optical purity is 98%.
Example Embodiment
[0039] Example 2 Synthesis of Levocarnitine
[0040] Dissolve 24g (0.6mol) of sodium hydroxide in 600ml of 10% (1mol) trimethylamine aqueous solution, and slowly add dropwise to 84g (0.5mol) (R)-4-chloro-3-hydroxyl at 0-5°C -Ethyl butyrate is dissolved in a solution formed by 1000ml of chloroform, the dropping rate is controlled at 4-6ml / min, and the reaction is stirred at 0-5℃ for 15 hours, then gradually raised to room temperature, reacted for 24 hours, and separated For the organic phase, concentrate the aqueous phase, stir and add Ambertlite IR-120 resin, absorb for 30 minutes, wash the resin three times with purified water, then wash the product three times with 10% ammonia water, combine the aqueous ammonia solution, and concentrate to obtain a white solid Leo Carney Tine product 68.1g, yield 84.1%, [α] 20 = -29.5° (c = 1, H 2 O).
Example Embodiment
[0041] Example 3 Synthesis of (R)-4-chloro-3-hydroxy-butyric acid ethyl ester
[0042] Dissolve 165g (1mol) of ethyl 4-chloroacetoacetate in 300ml of ethanol, add it to the hydrogenation reactor, and then add 10g of L-tartaric acid modified Ni-B / SiO 2 Catalyst, seal the reactor, replace the air in the reactor with nitrogen, and then blow in hydrogen to replace the nitrogen, keep the pressure of the reactor at 12kg, then increase the temperature and control the reaction at 50℃, react for 6 hours, leave to cool, and concentrate the reaction mixture under reduced pressure , The concentrate is distilled under high vacuum, and the fraction at 70°C (about 0.5mmHg) is collected to obtain 157.5g of colorless transparent liquid (R)-4-chloro-3-hydroxy-butyric acid ethyl ester, yield: 94.5%, optical purity Is 97%.
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